Green sulfur dye and process of making same.



i forty grains of melt made from amidoazoben- UNITED STATES Patented June 23, 1903.

PATENT OFFICE.

EDWARD CULMANN, OF BUFFALO, NEW YORK, ASSIGNOR TO SOHOELLKOPF, HARTFORD & HANNA COMPANY, OF BUFFALO, NEW YORK.

GR EENISULFUR DYE AND PROCESS OF MAKING SAME.

fiPECIFICJ-LTION forming part of Letters Patent No. 731,669, dated June 23, 1903.

. Application filed September 30, 1902.

Improvement in Green Sulfur Dyes, of which the following is a specification.

, This invention has for its object to produce a green dyestuff from the hydrochloric-acid salts of amidoazobenzene or its homologue amidoazotoluene.

In practicing my invention the hydrochloric-acid salt of amidoazobenzene or amidoazotoluene is melted, together with para-amidophenol, in about equal parts for about three hours at a temperature of about 180 centigrade. The melt of amidoazobenzene hydrochlorid and para-amidophenol is soluble in a watery solution of caustic soda with a blue color, While the melt of amidoazotoluene hydrochlorid and para-amidophenol dissolves in the same solution with a reddish-violet color. By boiling either of these melts with sodium sulfid and sulfur a green dyestuff is produced which dyes cotton directly in a bath containing sodium sulfid. I prefer to add a copper salt, whereby a somewhat more brilliant dyestufi is produced.

For example, one hundred and forty grains of sodium sulfid, fifty-five grains of sulfur,

zene or amidoazotoluene and para-amidophen01, fourteen grains of copper sulfate, and

I one hundred and thirty cubic centimeters of water are heated, preferably under a return cooler, for about twenty-four hours at-a temperature of about 102 to 105 centigrade and are then evaporated to dryness.

The dyestuff so made from amidoazobenzene hydrochlorid and 'para-amidophenol dyes cotton in w a bath containing alkali sulfid a dark shade.

Russian green. T

of green similar to the shade usually called This dry color dissolves in water with a green color, and when an acid is added to this solution a dark-green precipitate is formed. This precipitate when dried dissolves in a solution of caustic soda Serial No. 125,437. (No specimens.)

with a blue-green color, in a solution of sodium sulfid with a dark-green color, and in concentrated sulfuric acid with a blue-black color. In a solution of carbonate of soda it is almost insoluble.

The dyestuif made as herein described from amidoazotoluene hydrochlorid and para-amidophenol dyes cotton olive green in a bath 5 5 containing an alkali sulfid. This dyestuff when evaporated to dryness dissolves in wa- I wish it to be understood that I do not limit myself to amidoazobenzene, but that its homologue amidoazotoluene isalso covered.

I claim as my invention 7 1. The process of manufacturing a green coloring-matter which consists in boiling a melt of the hydrochloric-acid salt of amidoazobenzene, and para-amidophenol with sodium sulfid and sulfur, substantially as set forth.

2. The process of manufacturing a green coloring-matter which consists in boiling a melt of the hydrochloric-acid salt of amidoazobenzene, with sodium sulfid, sulfur and a copper salt, substantially as set forth.

3. The herein-described green dyestuffs prepared by boiling a melt of the hydrochloric-acid salt of amidobenzene, with sodium sulfid and sulfur, said dyestuff being of green color, almost insoluble in a watery solution of carbonate of soda, soluble in sodium sulfid 8 5 with a green color and in concentrated sulfuric acid with a dark color, substantially as set forth.

Witness my hand this 26th day of September, 1902.

EDWARD CULMA'NN. Witnesses:

FRED C. BONNER, GEORGE MARQUARDT.

This dried precipitate dissolves 6o 

